Synthesis method of dihydroimidazole compound
A dihydroimidazole and synthesis method technology, applied in chemical instruments and methods, chemical/physical processes, chemical/physical/physical chemical processes, etc., can solve problems such as low reaction efficiency, cumbersome reaction steps, long reaction time, etc., to achieve The effect of speeding up the reaction rate, easy reaction process, and green reaction conditions
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Embodiment 1
[0041]Dissolve 1.5mmol (0.3915g) of (2E,4E)-4-(acetoxyimino)-4-phenylbut-2-enoic acid ethyl ester and 0.1mmol (0.0099g) of cuprous chloride in In 10mL of tetrahydrofuran, the resulting mixed solution was recorded as solution A; 1mmol (0.0930g) of aniline, 2mmol (0.0600g) of paraformaldehyde and 0.4mmol (0.0488g) of 4-methylaminopyridine were dissolved in 10mL of tetrahydrofuran to obtain The mixed solution is denoted as solution B, and then solution A and solution B are pumped in the microchannel reaction device according to the flow volume ratio of 1:1, and the flow rate is respectively 0.2mL / min, and enters the microchannel reactor after being mixed by the Y-type mixer ( The inner diameter of the polytetrafluoroethylene tube of the microreactor is 0.5mm, and the volume of the polytetrafluoroethylene tube is 4mL) to react at 130°C for 20min. The organic phase was obtained from the discharge of the microreactor, and the crude product was obtained by vacuum concentration, which...
Embodiment 2
[0043] 1.5mmol (0.4635g) of (2E,4E)-4-(acetoxyimino)-4-(4-methoxyphenyl)but-2-enoic acid ethyl ester, 0.1mmol (0.0099g) 1mmol (0.0930g) of aniline, 2mmol (0.0600g) of paraformaldehyde and 0.4mmol (0.0488g) of 4-methylaminopyridine were dissolved In 10mL of tetrahydrofuran, the resulting mixed solution is recorded as solution B, and then solution A and solution B are pumped into the microchannel reaction device according to the flow volume ratio of 1:1, the flow rate is 0.2mL / min respectively, and after being mixed by a Y-shaped mixer Enter the microchannel reactor (the inner diameter of the polytetrafluoroethylene tube of the microreactor is 0.5mm, the volume of the polytetrafluoroethylene tube is 4mL) and react at 130°C for 10min. The organic phase was obtained from the discharge of the microreactor, and the crude product was obtained by vacuum concentration, which was separated by developer column chromatography with a ratio of petroleum ether to ethyl acetate of 20:1 to obt...
Embodiment 3
[0045] 1.5mmol (0.4170g) of (2E,4E)-4-(acetoxyimino)-4-(4-fluorophenyl)but-2-enoic acid ethyl ester, 0.1mmol (0.0099g) of chlorine Cuprous chloride was dissolved in 10 mL of tetrahydrofuran, and the resulting mixed solution was recorded as solution A; 1 mmol (0.0930 g) of aniline, 2 mmol (0.0600 g) of paraformaldehyde and 0.4 mmol (0.0488 g) of 4-methylaminopyridine were dissolved in 10 mL In tetrahydrofuran, the resulting mixed solution is recorded as solution B, and then solution A and solution B are pumped into the microchannel reaction device according to the flow volume ratio of 1:1, and the flow rate is 0.2mL / min respectively. In the channel reactor (the inner diameter of the polytetrafluoroethylene tube of the microreactor is 0.5 mm, and the volume of the polytetrafluoroethylene tube is 4 mL), react at 130° C. for 10 min. The organic phase was obtained from the discharge of the microreactor, and the crude product was obtained by vacuum concentration, which was separated...
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